CN107841340B - A kind of method that triglycerides thermochemical study prepares biological aviation hydrocarbon fuel - Google Patents
A kind of method that triglycerides thermochemical study prepares biological aviation hydrocarbon fuel Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G69/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one other conversion process
- C10G69/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one other conversion process plural serial stages only
- C10G69/04—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one other conversion process plural serial stages only including at least one step of catalytic cracking in the absence of hydrogen
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Abstract
A kind of method that triglycerides thermochemical study prepares biological aviation hydrocarbon fuel, catalytic pyrolysis: triglycerides and basic catalyst are added in cracking reaction kettle, carry out catalytic pyrolysis, obtain cracked oil；Air-distillation: gained cracked oil is added in three-necked flask, carries out air-distillation, collects fraction；Aromatisation: gained fraction and aromatized catalyst are added in autoclave, open stirring, and heating reaction after reaction, is centrifuged off catalyst, obtains using alkane and aromatic hydrocarbons as the aviation hydrocarbon fuel component of main component；Add hydrogen: aviation hydrocarbon fuel component and hydrogenation catalyst are added in autoclave, be passed through hydrogen, opens stirring, heating reaction；After reaction, catalyst is filtered out, is obtained with alkane, aromatic hydrocarbon and cycloalkane as main part liquid mixture, as biological aviation hydrocarbon fuel.Hydrocarbon fuel produced by the invention is the mixture of alkane, aromatic hydrocarbon and cycloalkane, and identical as Aviation Fuel component, property is close.
Description
Technical field
The invention belongs to biomass energy higher value application fields, and in particular to triglycerides thermochemical study preparation biology
The method of aviation hydrocarbon fuel.
Background technique
Currently, the Aviation Fuel in China is all from petrochemical refining, but Aviation Fuel yield component only accounts for crude oil total amount
10% or so.Aviation Fuel is the important leverage for developing China's civil aviation.In the increasingly depleted and carbon emission reduction of petroleum resources
Under dual-pressure, alternative biological Aviation Fuel is developed as raw material using biomass and is attracted extensive attention.Triglycerides is as life
The main component of object grease (vegetable oil and animal tallow), compared with other biological matter, chemical structure and petroleum are more close.
The most common transform mode of triglycerides is ester-interchange method biodiesel for automobile.The main composition of biodiesel is fatty acid
Methyl esters differs larger with petrochemical industry fuel components, and its low temperature flow is poor, and high oxygen content, calorific value is low, fires far from aviation is reached
The use standard of oil.
The catalytic pyrolysis of bio-oil is the another important channel for producing regeneratable liquors fuel.The catalyst mainly used
There are aluminium oxide, molecular sieve and basic catalyst.It is wherein higher as the fuel oil acid value of catalyst preparation using aluminium oxide and molecular sieve,
Low temperature flow is poor.Moreover, using molecular sieve as the pyrolysis product of catalyst, the predominantly fragrance of the C6-C9 of gasoline component range
The hydro carbons of hydrocarbon or the C12-C18 of diesel component range is not able to satisfy Aviation Fuel molecular weight distribution in the requirement of C8-C15.With alkali
Property oxide be catalyst preparation liquid fuel, main component be molecular weight distribution C8-C19 linear paraffin, aviation combustion
Oil is using alkane, aromatic hydrocarbon and cycloalkane as the mixture of main component, and single molecular structure is not able to satisfy aviation fuel
Demand also needs to carry out further molecular weight and molecular structure to Pyrolysis fuel oil PFO.In addition, the fuel oil of base catalysis cracking
Although acid value is lower, is used for Aviation Fuel, still need to further decrease acid value.
Summary of the invention
The technical issues of solution: in order to solve in existing cracked oil there are partial fatty acid, the single problem of molecular structure,
The present invention provides a kind of methods of triglycerides thermochemical study preparation aviation hydrocarbon fuel.The hydrocarbon fuel of production is alkane
The mixture of hydrocarbon, aromatic hydrocarbon and cycloalkane, identical as Aviation Fuel component, property is close.
Technical solution: a kind of method that triglycerides thermochemical study prepares biological aviation hydrocarbon fuel, including following step
Rapid: the first step, catalytic pyrolysis: triglycerides and basic catalyst are added in cracking reaction kettle, and the basic catalyst adds
Enter 5~20wt.% that amount accounts for triglycerides；At 350 DEG C~450 DEG C of temperature of reaction kettle, 260 DEG C~320 DEG C of rectifying column temperature
Under the conditions of, catalytic pyrolysis is carried out, cracked oil is obtained；Second step, air-distillation: gained cracked oil is added in three-necked flask, into
90 DEG C~270 DEG C of fraction is collected in row air-distillation；Third step, aromatisation: by fraction obtained by previous step and aromatized catalyst
It is added in autoclave, the additional amount of the aromatized catalyst is 5~15wt.% of fraction；Stirring is opened, will be reacted
Kettle temperature degree is increased to 300 DEG C~350 DEG C, and 2~8h of reaction time is centrifuged off catalyst after reaction, obtain with alkane and
Aromatic hydrocarbons is the liquid fuel of main component；4th step, adds hydrogen: liquid fuel obtained by previous step and hydrogenation catalyst are added to height
It presses in reaction kettle, the additional amount of the hydrogenation catalyst accounts for 1~10wt.% of fuel oil, is passed through 4~9MPa hydrogen, and unlatching is stirred
It mixes, temperature of reaction kettle is increased to 150 DEG C~250 DEG C, 2~8h of reaction time；After reaction, filter out catalyst, obtain with
Alkane, aromatic hydrocarbon and cycloalkane are main part liquid mixture, as biological aviation hydrocarbon fuel.
Above-mentioned triglycerides is any one in soybean oil, rubber seed oil, acidification oil or gutter oil.
Above-mentioned basic catalyst is alkali metal, alkaline earth oxide or alkaline earth metal hydroxide.
Above-mentioned basic catalyst is sodium carbonate, sodium hydroxide, potassium hydroxide, any one in calcium oxide.
Above-mentioned basic catalyst mass fraction accounts for the 10wt.% of triglycerides, and temperature of reaction kettle is 350 DEG C~420 DEG C, essence
280 DEG C~300 DEG C of column temperature.
Above-mentioned aromatized catalyst is any one in HZSM-5 and its modified molecular sieve catalyst.
Above-mentioned aromatized catalyst mass fraction is the 5~15wt.% for cracking oil distillate, and reaction temperature is 350 DEG C, reaction
Time is 6h.
Above-mentioned hydrogenation catalyst is Raney's nickel, any one in Pd/C, Pt/C, Rh/C.
The initial hydrogen pressure of above-mentioned hydrogenation reaction is 6MPa, and reaction temperature is 200 DEG C, reaction time 6h.
The utility model has the advantages that the present invention provides the sides that a kind of triglycerides thermochemical study prepares biological aviation hydrocarbon fuel
Method uses the acid value of part catalyst degradation cracked oil in cracking process.By air-distillation, extracting carbon chain lengths in cracked oil is
The group of C8-C15 is divided into aviation component.And by aromatization process, realizes alkene aromatisation and remaining carboxylic acid depickling, reduce cracking
The presence of labile element in oil, reduces acid value, improves aromatic hydrocarbon content.Hydrogenation reaction transform portion aromatic hydrocarbon is ring
Alkane is obtained using alkane, aromatic hydrocarbon and cycloalkane as the mixture of main component, and composition is consistent with Aviation Fuel composition, property
Matter is close.For bio-oil higher value application, it is converted into biological aviation hydrocarbon fuel and provides an effective way.
Detailed description of the invention
Fig. 1 is change of component figure during 1 thermochemical study of embodiment；
Fig. 2 is embodiment 1, embodiment 2, the cracked oil carbon chain length distribution figure of embodiment 3 and embodiment 4.
Specific embodiment
Below with reference to particular content of the invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts,
Belong to protection scope of the present invention.
A kind of method that triglycerides thermochemical study prepares biological aviation hydrocarbon fuel, comprising the following steps:
The first step triglycerides and basic catalyst is added in cracking reaction kettle, the additional amount of the basic catalyst
5~20wt.% of triglycerides is accounted for, controls 350 DEG C~450 DEG C of temperature of reaction kettle, the item that 260 DEG C~320 DEG C of rectifying column temperature
Under part, base catalysis cracking is carried out；Basic catalyst is alkali metal or alkaline earth oxide, hydroxide, can be carbonic acid
Sodium, sodium hydroxide, potassium hydroxide, any one in calcium oxide, preferably sodium carbonate.
Gained cracked oil is added in three-necked flask second step, carries out air-distillation, collects 90 DEG C~270 DEG C of fraction.
Normal pressure described in text refers to a standard atmospheric pressure.
Fraction obtained by previous step and aromatized catalyst are added in autoclave by third step, and the aromatisation is urged
The additional amount of agent is 5~15wt.% of fraction, opens stirring, and temperature of reaction kettle is increased to 300 DEG C~350 DEG C, when reaction
Between 2~8h be centrifuged off catalyst after reaction, obtain using alkane and aromatic hydrocarbons as the liquid-fuel oil of main component.
Liquid fuel material obtained by previous step and hydrogenation catalyst are added in autoclave by the 4th step, described plus hydrogen
The additional amount of catalyst accounts for 1~10wt.% of fuel oil, is passed through 4~9MPa hydrogen, and temperature of reaction kettle is increased to 150 DEG C -250
DEG C, 2~8h is reacted, catalyst is filtered out, obtains biological aviation hydrocarbon fuel.
Embodiment 1
The sodium carbonate of 1500g soybean oil and 10wt.% are added in cracking reaction kettle, stirring, rectifying column temperature liter are opened
Temperature is to 280 DEG C~300 DEG C, when reaction kettle is warming up to 350 DEG C, condensed fluid occurs, is gradually heated to 450 DEG C, keeps to without splitting
Solve liquid outflow.Air-distillation is carried out to cracking liquid, collects 90 DEG C~270 DEG C fractions.Take 80g fraction and 5wt.%HZSM-5
(Si/Al=27) catalyst opens stirring in autoclave, and reaction kettle is warming up to 350 DEG C, reacts 6h, is centrifuged off and urges
Agent.It takes 40g previous step product and 5wt.%Pd/C catalyst in autoclave, is passed through hydrogen 6MPa, open stirring, instead
It answers kettle to be warming up to 200 DEG C, reacts 6h, the mixture containing alkane, aromatic hydrocarbon and cycloalkane can be obtained, as biological aviation combustion
Oil.
Embodiment 2
The sodium carbonate of 1500g gutter oil and 5wt.% are added in cracking reaction kettle, stirring, the heating of rectifying column temperature are opened
To 280 DEG C~300 DEG C, when reaction kettle is warming up to 350 DEG C, there is condensed fluid, be gradually heated to 450 DEG C, keeps to no cracking
Liquid outflow.Air-distillation is carried out to cracking liquid, collects 90 DEG C~270 DEG C fractions.Take 80g fraction and 5wt.%HZSM-5
(Si/Al=27) catalyst opens stirring in autoclave, and reaction kettle is warming up to 350 DEG C, reacts 8h, is centrifuged off and urges
Agent.It takes 40g previous step product and 5wt.%Pd/C catalyst in autoclave, is passed through hydrogen 6MPa, open stirring, instead
It answers kettle to be warming up to 200 DEG C, reacts 6h, the mixture containing alkane, aromatic hydrocarbon and cycloalkane can be obtained, as biological aviation combustion
Oil.
The sodium carbonate of 1500g soybean oil and 5wt.% are added in cracking reaction kettle, stirring, the heating of rectifying column temperature are opened
To 260 DEG C~280 DEG C, when reaction kettle is warming up to 350 DEG C, there is condensed fluid, be gradually heated to 420 DEG C, keeps to no cracking
Liquid outflow.Air-distillation is carried out to cracking liquid, collects 90 DEG C~270 DEG C fractions.Take 80g fraction and 5wt.%HZSM-5
(Si/Al=27) catalyst opens stirring in autoclave, and reaction kettle is warming up to 350 DEG C, reacts 2h, is centrifuged off and urges
Agent.It takes 40g previous step product and 5wt.%Pd/C catalyst in autoclave, is passed through hydrogen 4MPa, open stirring, instead
It answers kettle to be warming up to 200 DEG C, reacts 4h, the mixture containing alkane, aromatic hydrocarbon and cycloalkane can be obtained, as biological aviation combustion
Oil.
Embodiment 4
The sodium carbonate of 1500g soybean oil and 10wt.% are added in cracking reaction kettle, stirring, rectifying column temperature liter are opened
Temperature is to 260 DEG C~280 DEG C, when reaction kettle is warming up to 350 DEG C, condensed fluid occurs, is gradually heated to 420 DEG C, keeps to without splitting
Solve liquid outflow.Air-distillation is carried out to cracking liquid, collects 90 DEG C~270 DEG C fractions.Take 80g fraction and 15wt.%HZSM-
5 (Si/Al=27) catalyst open stirring in autoclave, and reaction kettle is warming up to 300 DEG C, react 4h, are centrifuged off and urge
Agent.It takes 40g previous step product and 10wt.%Pd/C catalyst in autoclave, is passed through hydrogen 9MPa, open stirring,
Reaction kettle is warming up to 200 DEG C, reacts 6h, the mixture containing alkane, aromatic hydrocarbon and cycloalkane can be obtained, as biological aviation
Fuel oil.
Embodiment 5
The sodium carbonate of 1500g soybean oil and 15wt.% are added in cracking reaction kettle, stirring, rectifying column temperature liter are opened
Temperature is to 300 DEG C~320 DEG C, when reaction kettle is warming up to 350 DEG C, condensed fluid occurs, is gradually heated to 420 DEG C, keeps to without splitting
Solve liquid outflow.Air-distillation is carried out to cracking liquid, collects 90 DEG C~270 DEG C fractions.Take 80g fraction and 10wt.%HZSM-
5 (Si/Al=27) catalyst open stirring in autoclave, and reaction kettle is warming up to 320 DEG C, react 6h, are centrifuged off and urge
Agent.It takes 40g previous step product and 1wt.%Pd/C catalyst in autoclave, is passed through hydrogen 9MPa, open stirring, instead
It answers kettle to be warming up to 200 DEG C, reacts 8h, the mixture containing alkane, aromatic hydrocarbon and cycloalkane can be obtained, as biological aviation combustion
Oil.
Embodiment 6
The sodium carbonate of 1500g soybean oil and 5wt.% are added in cracking reaction kettle, stirring, the heating of rectifying column temperature are opened
To 300 DEG C~320 DEG C, when reaction kettle is warming up to 350 DEG C, there is condensed fluid, be gradually heated to 450 DEG C, keeps to no cracking
Liquid outflow.Air-distillation is carried out to cracking liquid, collects 90 DEG C~270 DEG C fractions.Take 80g fraction and 5wt.%HZSM-5
(Si/Al=27) catalyst opens stirring in autoclave, and reaction kettle is warming up to 350 DEG C, reacts 4h, is centrifuged off and urges
Agent.It takes 40g previous step product and 5wt.%Pd/C catalyst in autoclave, is passed through hydrogen 6MPa, open stirring, instead
It answers kettle to be warming up to 200 DEG C, reacts 2h, the mixture containing alkane, aromatic hydrocarbon and cycloalkane can be obtained, as biological aviation combustion
Oil.
Embodiment 7
The calcium oxide of 1500g soybean oil and 5wt.% are added in cracking reaction kettle, stirring, the heating of rectifying column temperature are opened
To 280 DEG C~300 DEG C, when reaction kettle is warming up to 350 DEG C, there is condensed fluid, be gradually heated to 450 DEG C, keeps to no cracking
Liquid outflow.Air-distillation is carried out to cracking liquid, collects 90 DEG C~270 DEG C fractions.Take 80g fraction and 5wt.%HZSM-5
(Si/Al=50) catalyst opens stirring in autoclave, and reaction kettle is warming up to 350 DEG C, reacts 6h, is centrifuged off and urges
Agent.It takes 40g previous step product and 5wt.%Pd/C catalyst in autoclave, is passed through hydrogen 6MPa, open stirring, instead
It answers kettle to be warming up to 200 DEG C, reacts 6h, the mixture containing alkane, aromatic hydrocarbon and cycloalkane can be obtained, as biological aviation combustion
Oil.
Embodiment 8
The sodium carbonate of 1500g soybean oil and 5wt.% are added in cracking reaction kettle, stirring, the heating of rectifying column temperature are opened
To 280 DEG C~300 DEG C, when reaction kettle is warming up to 350 DEG C, there is condensed fluid, be gradually heated to 450 DEG C, keeps to no cracking
Liquid outflow.Air-distillation is carried out to cracking liquid, collects 90 DEG C~270 DEG C fractions.Take 80g fraction and 5wt.%HZSM-5
(Si/Al=27) catalyst opens stirring in autoclave, and reaction kettle is warming up to 350 DEG C, reacts 6h, is centrifuged off and urges
Agent.It takes 40g previous step product and 10wt.% Raney's nickel catalyst in autoclave, is passed through hydrogen 9MPa, unlatching is stirred
It mixes, reaction kettle is warming up to 200 DEG C, reacts 6h, the mixture containing alkane, aromatic hydrocarbon and cycloalkane can be obtained, as biological
Aviation Fuel.
Embodiment 9
The sodium carbonate of 1500g soybean oil and 20wt.% are added in cracking reaction kettle, stirring, rectifying column temperature liter are opened
Temperature is to 280 DEG C~300 DEG C, when reaction kettle is warming up to 350 DEG C, condensed fluid occurs, is gradually heated to 450 DEG C, keeps to without splitting
Solve liquid outflow.Air-distillation is carried out to cracking liquid, collects 90 DEG C~270 DEG C fractions.Take 80g fraction and 5wt.%HZSM-5
(Si/Al=27) catalyst opens stirring in autoclave, and reaction kettle is warming up to 320 DEG C, reacts 6h, is centrifuged off and urges
Agent.It takes 40g previous step product and 5wt.% Raney's nickel catalyst in autoclave, is passed through hydrogen 9MPa, open stirring,
Reaction kettle is warming up to 150 DEG C, reacts 6h, the mixture containing alkane, aromatic hydrocarbon and cycloalkane can be obtained, as biological aviation
Fuel oil.
The result that base catalysis cracks in 1 embodiment of table
Change of component in reaction process in 2 embodiment 1 of table
Change of component in reaction process in 3 embodiment 2 of table
Fuel oil nature is compared with national standard Air China air-fuel oil nature in 4 embodiment 1 of table
A refers to GB/T 6537-2006.
Claims (1)
1. a kind of method that triglycerides thermochemical study prepares biological aviation hydrocarbon fuel, it is characterised in that including following step
It is rapid: the sodium carbonate of 1500 g soybean oils and 10 wt.% being added in cracking reaction kettle, stirring is opened, rectifying column temperature is warming up to
280 DEG C ~ 300 DEG C, when reaction kettle is warming up to 350 DEG C, there is condensed fluid, be gradually heated to 450 DEG C, keeps to no cracking
Liquid outflow；Air-distillation is carried out to cracking liquid, collects 90 DEG C ~ 270 DEG C fractions；Take 80 g fractions and 5 wt.% Si/Al
=27 HZSM-5 catalyst opens stirring in autoclave, and reaction kettle is warming up to 350 DEG C, reacts 6 h, is centrifuged off
Catalyst；It takes 40 g previous step products and 5 wt.% Pd/C catalyst in autoclave, is passed through 6 MPa of hydrogen, open
Stirring, reaction kettle are warming up to 200 DEG C, react 6 h, the mixture containing alkane, aromatic hydrocarbon and cycloalkane can be obtained, as
Biological Aviation Fuel.
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| CN110257098A (en) * | 2019-06-25 | 2019-09-20 | 中国林业科学研究院林产化学工业研究所 | A kind of method that bio-oil thermochemical study reduces reaction activity preparation biological Aviation Fuel and biodiesel |
| CN110835545A (en) * | 2019-11-01 | 2020-02-25 | 济宁市产品质量监督检验所 | Method for preparing hydrocarbon fuel oil by controlling molecular mass of grease cracking oil through reactive distillation |
| CN112410118A (en) * | 2020-10-30 | 2021-02-26 | 中国林业科学研究院林产化学工业研究所 | Thermochemical pretreatment method for waste grease or soapstock |
| CN113444538B (en) * | 2021-06-24 | 2022-08-05 | 中国林业科学研究院林产化学工业研究所 | Method for desulfurizing illegal cooking oil through thermochemical pretreatment of copper nitrate |
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